Electric Literature of 7664-66-6, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 7664-66-6 as follows.
Phenyl chloroformate (15.2 kg, 97.1 mol) was dissolved in toluene (115.7 kg) and cooled to 3 C. 4-isopro- poxyaniline (III) (13.3 kg, 88.0 mol) was mixed with acetonitrile (43.4kg) and slowly added to the phenyl chloroformate solution over 1 hour 40 minutes, followed by slow addition of triethylamine (9.8kg, 96.8 mol) over 46 minutes. The mixture was heated to 17.5C. and stirred for 3 hours 30 minutes until the reaction was deemed complete by HPLC. The product solution was washed with iN HC1, followed by removing acetonitrile though an azeotropic distillation with additional toluene (52.3 kg). The solution was heated to 58 C. before slowly adding heptane (43.7 kg) over 1 hour 2 minutes, after which the slurry was cooled to 23.5 C. over 2 hours 35 minutes and stirred for an additional 2 hours 51 minutes. The material was isolated, washed twice with heptane, and dried at 40 C. for 3 hours 49 minutes. The product was discharged, yielding 19.1 kg of the title compound (lIla) (80% yield, 100% purity HPLC AUC). ?H NMR (300 MHz, CD3OD, oe): 7.38 (m, 4H), 7.19 (m, 3H), 6.86 (d, J=9 Hz 2H), 4.52 (sept, J=6 Hz, 1H), 1.28 (d, J=6 Hz, 611).
According to the analysis of related databases, 7664-66-6, the application of this compound in the production field has become more and more popular.
Reference:
Patent; Millennium Phamaceuticals, Inc.; Armitage, Ian; Ferdous, Abu J.; Bourland, Michael E.; Boyle, Craig S.J.; Cooper, Martin Ian; Langston, Marianne; US2015/133460; (2015); A1;,
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